CN114850219A - Preparation method of high-precision thin-diameter thin-wall nickel-titanium alloy pipe - Google Patents
Preparation method of high-precision thin-diameter thin-wall nickel-titanium alloy pipe Download PDFInfo
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- CN114850219A CN114850219A CN202210373784.7A CN202210373784A CN114850219A CN 114850219 A CN114850219 A CN 114850219A CN 202210373784 A CN202210373784 A CN 202210373784A CN 114850219 A CN114850219 A CN 114850219A
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- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 91
- 238000005096 rolling process Methods 0.000 claims abstract description 70
- 238000010622 cold drawing Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 20
- 239000000314 lubricant Substances 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000011265 semifinished product Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001103 M42 high speed steel Inorganic materials 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005553 drilling Methods 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000000446 fuel Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000004519 grease Substances 0.000 claims description 5
- 230000001050 lubricating effect Effects 0.000 claims description 5
- 229910000997 High-speed steel Inorganic materials 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 230000007547 defect Effects 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000003672 processing method Methods 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 2
- 238000005242 forging Methods 0.000 description 5
- 238000001192 hot extrusion Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005097 cold rolling Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 1
- 210000000038 chest Anatomy 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 238000000886 hydrostatic extrusion Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- HLXZNVUGXRDIFK-UHFFFAOYSA-N nickel titanium Chemical compound [Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ti].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni].[Ni] HLXZNVUGXRDIFK-UHFFFAOYSA-N 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B17/00—Tube-rolling by rollers of which the axes are arranged essentially perpendicular to the axis of the work, e.g. "axial" tube-rolling
- B21B17/02—Tube-rolling by rollers of which the axes are arranged essentially perpendicular to the axis of the work, e.g. "axial" tube-rolling with mandrel, i.e. the mandrel rod contacts the rolled tube over the rod length
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
- B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
- B21B45/0239—Lubricating
- B21B45/0242—Lubricants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/16—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes
- B21C1/22—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles
- B21C1/24—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles by means of mandrels
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a preparation method of a high-precision thin-diameter thin-wall nickel-titanium alloy pipe, which comprises the following steps: firstly, preparing a tube blank; secondly, warm rolling the tube blank to obtain a semi-finished tube; and thirdly, cold drawing the pipe to obtain a finished pipe. The invention adopts warm rolling to obtain a semi-finished pipe, the problem of difficult deformation of the nickel-titanium alloy can be fundamentally solved in the warm rolling process, the plastic processing performance of the material is improved, the surface quality of the rolled pipe is good, and the cracking defect is avoided, and compared with a cold processing method, the intermediate annealing frequency in the rolling process can be obviously reduced, thereby being beneficial to improving the production efficiency and reducing the production cost; the problem of poor cold processing plasticity of the nickel-titanium alloy is solved, the obtained pipe has good surface quality and dimensional precision, high yield and low cost, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a preparation method of a high-precision thin-diameter thin-wall nickel-titanium alloy pipe.
Background
Nitinol is the largest-used and most versatile shape memory alloy developed in recent decades. Compared with traditional medical metal materials (such as stainless steel, titanium alloy and the like), the nickel-titanium alloy has unique shape memory effect and superelasticity, better corrosion resistance and wear resistance and excellent mechanical property, and is widely applied to the fields of oral cavity, orthopedics, cardiovascular and cerebrovascular, liver, gall bladder, chest and the like.
The high-precision thin-diameter thin-wall nickel-titanium alloy pipe with the diameter of 2 mm-3 mm (tolerance +/-0.02 mm) and the wall thickness of 0.2 mm-0.3 mm (tolerance +/-0.02 mm) has high strength, radial supporting force and special shape recovery capability, and is widely applied to minimally invasive surgical instruments, particularly to interventional intracavity stents. However, the nickel-titanium alloy has large deformation resistance at room temperature, high work hardening rate and poor plastic deformation capability, and the pipe is easy to crack in the cold deformation process, so the forming problem of the alloy pipe is always a difficult point in the field of plastic processing.
At present, the method for producing the nickel-titanium alloy pipe in China mainly adopts a method of combining cold machining with multi-pass annealing, and has low production efficiency and high production cost. For example, the technological process adopted in the reference (Hujie, Liuli. titanium-nickel shape memory alloy capillary processing technology research [ J ]. New technology and New technology, 2006, 6: 51-52.) is as follows: vacuum smelting, forging, medium-temperature hydrostatic extrusion of a pipe blank, cold rolling, cold drawing and heat treatment. However, because the alloy has a very fast work hardening rate, a large number of transverse cracks are easy to appear on the inner surface and the outer surface of the pipe in the cold rolling process, particularly on the most obvious inner surface, and the rolled pipe is usually broken.
Some patents adopt hot working method to prepare nickel-titanium alloy tube. Chinese patent CN103394532B adopts induction heating to realize continuous hot drawing of the nickel-titanium alloy tube, but the induction heating process can cause uneven heating of the tube. The Chinese patent CN1686627A inserts the core rod into the nickel-titanium alloy tube blank, then adopts continuous hot drawing to draw the combination body, and finally takes out the core rod to obtain the alloy thin-wall tube. Although the hot drawing method can improve the plasticity of the nickel-titanium alloy, the inner part and the surface of the pipe prepared by the method are in a hot processing state, the precision and the quality of the pipe are not high, and the requirements of the implanted stent on the size and the precision of the pipe are difficult to meet. In addition, the mandrel needs to be inserted into the nickel-titanium alloy tube blank in the existing hot drawing process of the nickel-titanium alloy tube, then the combined body is drawn, and the mandrel needs to be taken out after the drawing is finished, so that the production flow is increased, the chemical components of the tube can be polluted, and the inner surface quality of the tube is poor.
At present, only a few companies in the United states and the French can realize the industrialization of the pipes, the production process of the domestic prior art is more and fussy, the production cost is high, the capacity of producing high-precision thin-diameter thin-wall nickel-titanium alloy pipes in a large scale is not realized, and the pipes still need to be imported in large quantity at present. Therefore, a new process for producing and processing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is actively developed, the production cost is reduced, the production efficiency is improved, and the method has great significance and wide application prospect.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a thin-wall nickel-titanium alloy pipe with high precision and small diameter aiming at the defects of the prior art. The method solves the problem of poor cold processing plasticity of the nickel-titanium alloy, and the obtained pipe has good surface quality and dimensional precision, high yield and low cost, and is suitable for large-scale industrial production.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized by comprising the following steps:
step one, preparing a tube blank: peeling a nickel-titanium alloy bar and then drilling to prepare a tube blank with the outer diameter less than or equal to 30mm and the wall thickness less than or equal to 5 mm;
step two, lubricating the surface of the tube blank: heating the surface of the tube blank in the step one by using a hydrogen flame heating gun to enable the surface temperature of the tube blank to reach 700-800 ℃ so as to remove redundant grease on the surface, and then placing the tube blank in the atmosphere for natural cooling; when the surface temperature of the tube blank is reduced by 300-400 ℃, uniformly coating a graphite emulsion lubricant on the inner surface and the outer surface of the tube blank, and then placing the tube blank in the atmosphere for natural air drying for later use;
step three, warm rolling the tube blank: penetrating the air-dried tube blank in the step two into a rolling mill mandrel, heating the tube blank to 500-700 ℃, and then starting rolling to obtain a semi-finished tube;
step four, cold drawing of the pipe: and D, performing cold drawing on the semi-finished pipe in the step II to obtain a finished pipe.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that in the step one, the nickel-titanium alloy bar is a hot extrusion bar or a hot forging bar.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the fuel used for heating in the second step is compressed hydrogen, and the flame size can be adjusted by controlling the ratio of the compressed hydrogen to the compressed air.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the core rod and the roller rolled in the third step are both made of M42 high-speed steel or W18Cr4V tungsten high-speed steel.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the rolling speed of the rolling in the third step is 100-500 mm/min, the feeding speed of a rolling mill is 2-6 mm/time, the processing rate of the rolling pass is less than or equal to 30%, the pipe is subjected to intermediate annealing treatment every 1-3 passes in the rolling process, the annealing temperature is 800-900 ℃, the annealing time is 30-90 min, and after the intermediate annealing is finished every time, the pipe is subjected to alkali washing and acid washing to remove a surface lubricant and an oxide layer; and after the final rolling, carrying out annealing treatment on the semi-finished product, wherein the annealing treatment temperature of the semi-finished product is 800-900 ℃, the annealing time is 30-90 min, and carrying out alkali washing and acid washing on the pipe to remove the surface lubricant and the oxide layer before the annealing treatment of the semi-finished product.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the warm rolling process comprises the following steps: when the outer diameter of the pipe is less than 30mm and more than 15mm, the warm rolling speed is not more than 300mm/min, and the feeding speed of the rolling mill is not more than 4 mm/time; when the outer diameter of the pipe is less than 15mm, the warm rolling speed is not more than 500mm/min, and the feeding speed of the rolling mill is not more than 6 mm/time.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the intermediate annealing treatment mode is electric contact heating annealing, and argon is adopted for protection in the annealing process; the mode of the semi-finished product annealing treatment is vacuum annealing.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the outer diameter of the semi-finished pipe in the third step is 4-6 mm, and the wall thickness is 0.4-0.6 mm; in the fourth step, the outer diameter of the finished pipe is 2 mm-3 mm, and the wall thickness is 0.2 mm-0.3 mm.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that in the fourth step, the cold drawing pass is not less than 5 times, the speed is 1-5 mm/s, the pass processing rate is not more than 20%, the pipe needs to be subjected to intermediate annealing treatment every 1-2 passes in the drawing process, the annealing temperature is 800-900 ℃, and the annealing time is 30-90 min.
The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized in that the cold drawing in the fourth step adopts moving core drawing.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts warm rolling to obtain the semi-finished pipe, the problem of difficult deformation of the nickel-titanium alloy can be fundamentally solved in the warm rolling process, the plastic processing performance of the material is improved, the rolled pipe has good surface quality and no cracking defect, and compared with a cold processing method, the invention can obviously reduce the intermediate annealing times in the rolling process, is beneficial to improving the production efficiency and reducing the production cost.
2. The invention adopts the moving core drawing method to prepare the finished pipe, the force balance established by the special appearance of the core in the drawing process is stabilized in the die hole, and the invention is very beneficial to improving the drawing productivity, the yield and the inner surface quality of the pipe. The prepared finished pipe has good surface quality and surface precision and high yield, can meet the use requirement of medical pipes, and is suitable for large-scale industrial production.
3. The invention can realize cogging rolling of the pipe blank with the outer diameter not larger than 30mm, and the drawing processing method is difficult to draw the large-specification pipe, so the method has low requirements on the size and the specification of the raw material pipe blank and can reduce the preparation cost of the pipe blank.
4. In the warm rolling process, the intermediate annealing is preferably selected from electric contact heating annealing, the electric contact heating temperature rise is fast, the temperature difference inside the heating material is small, the annealed tissue is uniform, the production efficiency can be further improved, and the production cost is reduced.
5. In the warm rolling process, the preferable materials of the mandrel and the roller are M42 high-speed steel or W18Cr4V tungsten high-speed steel, the high-temperature hardness of the mandrel and the roller is high, the deformation of the mandrel and the roller in the warm rolling process is small, and the service life and the rolling precision of the mandrel and the roller are ensured.
The technical solution of the present invention is further described in detail by examples below.
Drawings
FIG. 1 is a photograph of the microstructure of the outer surface of the finished pipe of example 1.
Fig. 2 is a photograph of the microstructure of the inner surface of the finished tube in example 1.
Fig. 3 is a photograph of the microstructure of the outer surface of the finished tubing of example 2.
Fig. 4 is a photograph of the microstructure of the inner surface of the finished tube in example 2.
Detailed Description
Example 1
Step one, preparing a tube blank: peeling a nickel-titanium alloy bar and then drilling a hole to prepare a nickel-titanium alloy tube blank with the outer diameter of 30mm and the wall thickness of 5mm, wherein the inner surface and the outer surface of the tube blank are smooth and have no visible defects; the nickel-titanium alloy bar is a hot extrusion bar or a hot forging bar;
step two, lubricating the surface of the tube blank: firstly, opening a hydrogen flame heating gun, heating the surface of the nickel-titanium alloy tube blank in the step one to 700 ℃ by using compressed hydrogen as fuel to remove redundant grease on the surface, and then placing the tube blank in the atmosphere for natural cooling; uniformly coating a graphite emulsion lubricant on the inner surface and the outer surface of the tube blank when the surface temperature of the tube blank reaches 300 ℃, and then placing the tube blank in the atmosphere for natural air drying for later use;
step three, warm rolling the tube blank: the materials of the warm-rolled core rod and the roll are both M42 high-speed steel (the nominal composition is W2Mo9Cr4VCo 8); the air-dried pipe blank is inserted into a core rod of a rolling mill, the pipe blank is heated to 700 ℃, then the rolling mill is started to carry out warm rolling, the processing rate of the rolling pass is less than or equal to 30%, in the rolling process, when the outer diameter of the pipe is less than 30mm and more than 15mm, the warm rolling speed is 300mm/min, the feeding speed of the rolling mill is 4 mm/time, when the outer diameter of the pipe is less than 15mm, the warm rolling speed is 500mm/min, and the feeding speed of the rolling mill is 6 mm/time; the specific rolling process comprises the following steps:
the intermediate annealing treatment mode is electric contact heating annealing, the annealing temperature is 900 ℃, the annealing time is 30min, argon protection is adopted in the annealing process, and after the annealing is finished, the tube is subjected to alkali washing and acid washing to remove a surface lubricant and an oxide layer; the annealing mode of the semi-finished product is vacuum annealing, the annealing temperature is 900 ℃, the annealing time is 30min, the tube is subjected to alkali washing and acid washing before annealing to remove a surface lubricant and an oxide layer, and the specification of the tube is obtained after the annealing is finished
The semi-finished pipe;
step four, cold drawing of the pipe: and (3) carrying out cold drawing on the semi-finished pipe in the third step, wherein the cold drawing method is moving core drawing, the drawing speed is 1mm/s, the pass processing rate is less than or equal to 20%, intermediate annealing treatment needs to be carried out on the pipe every 1-2 passes in the drawing process, and the specific drawing process is as follows:
the annealing process is vacuum annealing, the annealing temperature is 900 ℃, and the annealing time is 30 min. And (3) obtaining a finished pipe after the annealing is finished, wherein the microstructures of the inner surface and the outer surface of the pipe are shown in figures 1 and 2, and the microstructures of the inner surface and the outer surface of the finished pipe are uniform and have no obvious defects.
The diameter of the finished pipe prepared by the embodiment is 3mm (tolerance +/-0.02 mm), the wall thickness is 0.3mm (tolerance +/-0.02 mm), the use requirement of the medical pipe can be met, and the pipe has wide application prospect on minimally invasive surgical instruments, particularly interventional intracavity stents.
Example 2
Step one, preparing a tube blank: peeling a nickel-titanium alloy bar and then drilling to prepare a nickel-titanium alloy tube blank with the outer diameter of 18mm and the wall thickness of 2mm, wherein the inner surface and the outer surface of the tube blank are smooth and have no visible defects; the nickel-titanium alloy bar is a hot extrusion bar or a hot forging bar;
step two, lubricating the surface of the tube blank: and (3) firstly opening a hydrogen flame heating gun, heating the surface of the nickel-titanium alloy tube blank in the step one to 800 ℃ by using compressed hydrogen as fuel to remove redundant grease on the surface, and then placing the tube blank in the atmosphere for natural cooling. Uniformly coating a graphite emulsion lubricant on the inner surface and the outer surface of the tube blank when the surface temperature of the tube blank reaches 400 ℃, and then placing the tube blank in the atmosphere for natural air drying for later use;
step three, warm rolling the tube blank: the materials of the rolled core rod and the rolled roller are W18Cr4V tungsten high-speed steel; the air-dried pipe blank is inserted into a core rod of a rolling mill, the pipe blank is heated to the temperature of 650 ℃, the rolling mill is started to carry out warm rolling, the processing rate of the rolling pass is less than or equal to 30 percent, the warm rolling speed is 100mm/min and the feeding speed of the rolling mill is 2 mm/time when the outer diameter of the pipe is more than 15mm, and the warm rolling speed is 400mm/min and the feeding speed of the rolling mill is 4 mm/time when the outer diameter of the pipe is less than 15 mm; the specific rolling process comprises the following steps:
the intermediate annealing treatment mode is electric contact heating annealing, the annealing temperature is 800 ℃, the annealing time is 90min, argon protection is adopted in the annealing process, and after the annealing is finished, the tube is subjected to alkali washing and acid washing to remove a surface lubricant and an oxide layer; the annealing mode of the semi-finished product is vacuum annealing, the annealing temperature is 800 ℃, the annealing time is 90min, the tube is subjected to alkali washing and acid washing before annealing to remove a surface lubricant and an oxide layer, and the specification of the tube is obtained after the annealing is finished
The semi-finished pipe;
step four, cold drawing of the pipe: and (3) carrying out cold drawing on the semi-finished pipe in the third step, wherein the cold drawing method is moving core drawing, the drawing speed is 5mm/s, the pass processing rate is less than or equal to 20%, the pipe needs to be subjected to intermediate annealing treatment in each pass in the drawing process, and the specific drawing process is as follows:
the annealing process is vacuum annealing, the annealing temperature is 800 ℃, and the annealing time is 90 min. And (3) obtaining a finished pipe after the annealing is finished, wherein the microstructures of the inner surface and the outer surface of the pipe are shown in figures 3 and 4, and the microstructures of the inner surface and the outer surface of the finished pipe are uniform and have no obvious defects.
The diameter of the finished pipe prepared by the embodiment is 2mm (tolerance +/-0.02 mm), the wall thickness is 0.2mm (tolerance +/-0.02 mm), the use requirement of the medical pipe can be met, and the pipe has wide application prospect on minimally invasive surgical instruments, particularly interventional endoluminal stents.
Example 3
Step one, preparing a tube blank: peeling a nickel-titanium alloy bar and then drilling a hole to prepare a nickel-titanium alloy tube blank with the outer diameter of 15mm and the wall thickness of 1.5mm, wherein the inner surface and the outer surface of the tube blank are smooth and have no visible defects; the nickel-titanium alloy bar is a hot extrusion bar or a hot forging bar;
step two, lubricating the surface of the tube blank: firstly, opening a hydrogen flame heating gun, heating the surface of the nickel-titanium alloy tube blank in the step one to 750 ℃ by using compressed hydrogen as fuel to remove redundant grease on the surface, and then placing the tube blank in the atmosphere for natural cooling. Uniformly coating a graphite emulsion lubricant on the inner surface and the outer surface of the tube blank when the surface temperature of the tube blank reaches 350 ℃, and then placing the tube blank in the atmosphere for natural air drying for later use;
step three, warm rolling the tube blank: the materials of the warm-rolled core rod and the roll are both M42 high-speed steel (the nominal composition is W2Mo9Cr4VCo 8); and (3) penetrating the air-dried pipe blank into a rolling mill mandrel, heating the pipe blank to 500 ℃, starting the rolling mill to perform warm rolling, wherein the processing rate of rolling passes is less than or equal to 30%, the warm rolling speed is 500mm/min, and the feeding speed of the rolling mill is 6 mm/time in the rolling process. The specific rolling process comprises the following steps:
the intermediate annealing treatment mode is electric contact heating annealing, the annealing temperature is 850 ℃, the annealing time is 60min, argon protection is adopted in the annealing process, and after the annealing is finished, the tube is subjected to alkali washing and acid washing to remove a surface lubricant and an oxide layer; the annealing mode of the semi-finished product is vacuum annealing, the annealing temperature is 850 ℃, the annealing time is 60min, the tube is subjected to alkali washing and acid washing before annealing to remove a surface lubricant and an oxide layer, and the specification of the tube is obtained after the annealing is finished
The semi-finished pipe;
step four, cold drawing of the pipe: and (3) carrying out cold drawing on the semi-finished pipe in the third step, wherein the cold drawing method is moving core drawing, the drawing speed is 3mm/s, the pass processing rate is less than or equal to 20%, the pipe needs to be subjected to intermediate annealing treatment in each pass in the drawing process, and the specific drawing process is as follows:
the annealing process is vacuum annealing, the annealing temperature is 850 ℃, and the annealing time is 60 min. And (4) obtaining a finished product pipe after annealing, wherein the inner surface and the outer surface of the finished product pipe have no obvious defects and have uniform tissues.
The diameter of the finished pipe prepared by the embodiment is 2mm (tolerance +/-0.02 mm), the wall thickness is 0.2mm (tolerance +/-0.02 mm), the use requirement of the medical pipe can be met, and the pipe has wide application prospect on minimally invasive surgical instruments, particularly interventional endoluminal stents.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a high-precision thin-diameter thin-wall nickel-titanium alloy pipe is characterized by comprising the following steps:
step one, preparing a tube blank: peeling a nickel-titanium alloy bar and then drilling to prepare a tube blank with the outer diameter of less than or equal to 30mm and the wall thickness of less than or equal to 5 mm;
step two, lubricating the surface of the tube blank: heating the surface of the tube blank in the step one by using a hydrogen flame heating gun to enable the surface temperature of the tube blank to reach 700-800 ℃ so as to remove redundant grease on the surface, and then placing the tube blank in the atmosphere for natural cooling; when the surface temperature of the tube blank is reduced by 300-400 ℃, uniformly coating a graphite emulsion lubricant on the inner surface and the outer surface of the tube blank, and then placing the tube blank in the atmosphere for natural air drying for later use;
step three, warm rolling the tube blank: penetrating the air-dried tube blank in the step two into a rolling mill mandrel, heating the tube blank to 500-700 ℃, and then starting rolling to obtain a semi-finished tube;
step four, cold drawing of the pipe: and D, performing cold drawing on the semi-finished pipe in the step II to obtain a finished pipe.
2. The method for preparing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe according to claim 1, wherein the nickel-titanium alloy bar in the first step is a hot extruded bar or a hot forged bar.
3. The method for preparing the thin-walled nickel titanium alloy tubular product with high precision and small diameter according to claim 1, wherein the fuel used for heating in the second step is compressed hydrogen, and the flame size can be adjusted by controlling the ratio of the compressed hydrogen to the compressed air.
4. The method for preparing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe as claimed in claim 1, wherein the core rod and the roller rolled in the third step are both M42 high-speed steel or W18Cr4V tungsten high-speed steel.
5. The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe according to claim 1, characterized in that the rolling speed of the rolling in the third step is 100 mm/min-500 mm/min, the feeding speed of the rolling mill is 2 mm/time-6 mm/time, the processing rate of the rolling pass is less than or equal to 30%, the pipe is subjected to intermediate annealing treatment every 1-3 passes in the rolling process, the annealing temperature is 800-900 ℃, the annealing time is 30-90 min, and after the intermediate annealing is finished, the pipe is subjected to alkali washing and acid washing to remove a surface lubricant and an oxide layer; and after the final rolling, carrying out annealing treatment on the semi-finished product, wherein the annealing treatment temperature of the semi-finished product is 800-900 ℃, the annealing time is 30-90 min, and carrying out alkali washing and acid washing on the pipe to remove the surface lubricant and the oxide layer before the annealing treatment of the semi-finished product.
6. The preparation method of the high-precision thin-diameter thin-wall nickel-titanium alloy pipe material according to claim 5, wherein in the warm rolling process: when the outer diameter of the pipe is less than 30mm and more than 15mm, the warm rolling speed is not more than 300mm/min, and the feeding speed of the rolling mill is not more than 4 mm/time; when the outer diameter of the pipe is less than 15mm, the warm rolling speed is not more than 500mm/min, and the feeding speed of the rolling mill is not more than 6 mm/time.
7. The method for preparing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe as claimed in claim 5, wherein the intermediate annealing treatment mode is electric contact heating annealing, and argon gas is adopted for protection in the annealing process; the mode of the semi-finished product annealing treatment is vacuum annealing.
8. The method for preparing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe material according to claim 1, wherein in the third step, the outer diameter of the semi-finished pipe material is 4mm to 6mm, and the wall thickness is 0.4mm to 0.6 mm; in the fourth step, the outer diameter of the finished pipe is 2 mm-3 mm, and the wall thickness is 0.2 mm-0.3 mm.
9. The method for preparing the high-precision thin-diameter thin-wall nickel-titanium alloy pipe according to claim 1, wherein in the fourth step, the cold drawing passes are not less than 5 times, the speed is 1mm/s to 5mm/s, the pass processing rate is not more than 20%, the pipe needs to be subjected to intermediate annealing treatment every 1 to 2 passes in the drawing process, the annealing temperature is 800 ℃ to 900 ℃, and the annealing time is 30min to 90 min.
10. The method for preparing the thin-walled nickel titanium alloy tubular product with high precision and small diameter according to claim 1, wherein the cold drawing in the fourth step is drawing by using a traveling core.
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